TW201341507A - Phosphor and light emitting apparatus - Google Patents

Abstract

Provided is a phosphor which comprises alkali earth ions, Si ion, N ion and Tb ion. Tb ion is used as a luminescence center. The phosphor has broad emission bands after excitation. The phosphor of the present invention can be used for light an emitting apparatus.

Description

Fluorescent powder and illuminating device

The present invention relates to a phosphor powder, and more particularly to a phosphor powder suitable for use in a light emitting diode source.

Light Emitting Diode (LED) is a mercury-free environmentally friendly light source with low power consumption, high service life, fast response rate, no heat radiation, and small volume. In 1996, Nichia Corporation first announced the use of blue LEDs with yttrium aluminum garnet (YAG) yellow phosphor powder to produce white light. From then on, White Light Emitting Diode (WLED) was officially launched. Enter commercialization. Due to the vigorous development of related technology industries in recent years, the luminous efficiency and reliability of WLED products have been continuously improved. Therefore, with the development trend of energy saving and carbon reduction, WLED, which is known as a green energy source, will gradually replace traditional lighting equipment such as incandescent bulbs, and is widely used in general lighting equipment, displays, automobiles, electronics, communications and other industries.

The white light emitted by the WLED is a two-wavelength light, a three-wavelength light or a four-wavelength light in which a plurality of colors are mixed. At present, the production method of WLED includes: exciting yellow fluorescent powder with blue LED; exciting red and green fluorescent powder with blue LED; and exciting fluorescent powder of various colors with purple or ultraviolet LED (for example, disclosed in Chinese Patent I340480) Using two to four light-emitting diodes, by adjusting their individual brightness to mix to form white light; and so on. Among them, the blue light LED is used to excite the YAG phosphor powder to generate yellow light, and then the white light emitting diode produced by the combination of yellow light and blue light to produce white light has low cost and high efficiency, and is still the mainstream in the market. However, its color rendering cannot be compared with traditional light bulbs and power-saving bulbs. Therefore, to achieve warm white LEDs, red phosphor powder must be added. The blue LED with red and green fluorescent powder has improved color temperature and color rendering, and the efficiency is also good.

Fluorescent powders are common luminescent materials in which an inorganic phosphor system utilizes electronic transitions to produce fluorescence. When the phosphor powder is stimulated by light, the electrons are excited to the high-energy excitation state, and when returning to the original low-energy state, the energy is radiated in the form of light. The inorganic phosphor powder is mainly composed of a host lattice and an activator, and a co-activator or a sensitizer may be added as needed to enhance luminous efficiency. The activator acts as a luminescence center, and the host lattice transmits energy during the excitation process. By changing the combination of the host crystal and the activator, the wavelength of the light emitted by the phosphor powder can be changed to produce different luminescent colors. In addition, the chemical composition of the host lattice, the type and concentration of the activator, etc., all affect the luminous efficiency of the phosphor powder. Fluorescent materials have evolved from earlier, less stable sulfides to later cerium oxide (silicate) phosphors. In recent years, nitrogen/nitrogen oxide fluorescent materials have been quite popular.

Fluorescent powders commonly used at present include aluminum oxide phosphor powder, cerium oxide phosphor powder, and nitrogen/nitrogen oxide phosphor powder. YAG phosphor powder (mainly composed of Y ₃ Al ₅ O ₁₂ :Ce), which was proposed by Japan Nichia Corporation in 1996 (mainly composed of Y ₃ Al ₅ O ₁₂ :Ce), and TAG phosphor powder published by Osram, Germany in 1999 ( The phosphor powder disclosed in the main composition of Tb ₃ Al ₅ O ₁₂ :Ce) and the Chinese Patent No. I353377 is an aluminum oxide phosphor powder using cerium (Ce) as an activator. Furthermore, the Ba ₂ MgSi ₂ O ₇ :Eu phosphor powder proposed by GE in the United States in 1998 and the Chinese patent I306675 disclose the use of cerium (Ce), europium (Eu), manganese (Mn), etc. as activators. A light powder or the like is a cerium oxide fluorescent powder. In addition, since nitrides and nitrogen oxides have excellent thermal stability, good chemical stability, non-toxicity, and high strength, fluorescent powders with nitrogen oxides and nitrides as host crystal lattices have also been published. , as disclosed in U.S. Patent No. 6,649,946, U.S. Patent 6,632,379, U.S. Patent No. 7,193,358, U.S. Patent No. 7, 525, 127 and U.S. Patent No. 7,569,987, and U.S. Pat. However, in the general nitrogen/nitrogen oxide phosphor powder, if Tb (Terbium) is used as the activator, it is often affected by problems such as poor radiation peaks, poor efficiency, and lack of light color. Its application value. Therefore, there is still a need to develop a phosphor powder that can improve the lack of conventional technology and has high application value.

In view of the lack of prior art, the present invention provides a fluorescent powder suitable for use in a light-emitting device, particularly for a light-emitting diode light source, which meets the needs of industrial utilization.

The invention provides a phosphor powder comprising an alkaline earth ion, a Si ion, an N ion and a Tb ion, wherein the Tb ion is an illuminating center, and the fluorescent powder is excited by excitation light absorbable by Tb ions, and has a half height Radiation peaks with a width greater than 20 nanometers (nm). According to an embodiment of the invention, the phosphor powder is excited by excitation light absorbable by Tb ions, and has an emission peak with a full width at half maximum of more than 25 nm. According to a specific embodiment of the invention, the alkaline earth ion is Mg ion, Ca ion, Sr ion, Ba ion or a combination thereof. According to a specific embodiment of the invention, the phosphor powder is excited by excitation light having a wavelength of 250 to 600 nm and has an emission peak having a full width at half maximum of more than 20 nm. According to a specific embodiment of the invention, the phosphor powder is excited by excitation light having a wavelength of 350 to 600 nm and has an emission peak having a full width at half maximum of more than 20 nm.

According to an embodiment of the invention, the phosphor system is as shown in formula (I):

T _x E _y Si _z N _r Tb _a L _b M _c (I),

Wherein T is Mg, Ca, Sr or Ba; E is Mg, Ca, Ba, Ti, Cu, Zn, B, Al, In, Sn, Sb, Bi, Ga, Y, La or Lu; L is Li, Na or K; M is Ce, Pr, Nd, Pm, Sm, Eu, Gd, Dy, Ho, Er, Tm, Yb or Mn; and 1.4≦x≦2.6,0≦y≦0.5, 4.3≦z≦5.6 , 7.4≦r≦9, 0.01≦a≦0.5, 0≦b≦0.5,0≦c≦0.5.

According to a specific embodiment of the present invention, the phosphor powder represented by the formula (I) is excited by excitation light absorbable by Tb ions, and has an emission peak having a full width at half maximum of more than 20 nm. According to an embodiment of the invention, the phosphor powder of the formula (I) is excited by excitation light having a wavelength of 250 to 600 nm and has an emission peak having a full width at half maximum of more than 20 nm. According to an embodiment of the invention, the phosphor powder of the formula (I) is excited by excitation light having a wavelength of 350 to 600 nm and has an emission peak having a full width at half maximum of more than 20 nm.

According to an embodiment of the invention, the phosphor powder is excited by excitation light absorbable by Tb ions, and has an excitation peak with a full width at half maximum of more than 50 nm. In one embodiment, the integrated area of the excitation peak intensity of the phosphor powder of the present invention having a wavelength of 350 to 600 nm is greater than 0.1 times the integrated area of the excitation peak intensity of the wavelength of 200 to 350 nm.

According to a specific embodiment of the invention, the phosphor powder has an average particle diameter of from 0.01 micrometers (μm) to 50 μm.

The phosphor powder of the present invention is suitable for use in a light-emitting device, and is particularly suitable for use in a light-emitting diode. According to an embodiment of the invention, the illumination device comprises a light source.

The phosphor powder of the present invention is excited by excitation light and has a broad radiation peak. Therefore, the lack of efficiency of the conventional phosphor powder and the lack of adjustability of the light color can be improved, which is in line with the needs of the industry.

The embodiments of the present invention are described by way of specific examples, and those skilled in the art can understand the advantages and advantages of the present invention as disclosed in the present disclosure. The present invention may be embodied or applied in various other specific embodiments. The details of the present invention can be variously modified and changed without departing from the spirit and scope of the invention.

The singular <RTI ID=0.0>"1" </ RTI> </ RTI> and <RTIgt;

The term "or" as used in the specification and the scope of the appended claims generally includes the meaning of "and/or" unless otherwise indicated.

The present invention provides a phosphor powder comprising an alkaline earth ion, a Si ion, an N ion, and a Tb ion, wherein the Tb ion is an illuminating center. The phosphor powder is excited by excitation light absorbable by Tb ions, and has a radiation peak having a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably more than 50 nm.

Examples of alkaline earth ions include, but are not limited to, Mg ions, Ca ions, Sr ions, Ba ions, and combinations thereof. Preferably, the alkaline earth ions are Mg ions, Ca ions, Sr ions, Ba ions or a combination thereof.

According to an embodiment of the invention, the phosphor system is as shown in formula (I):

T _x E _y Si _z N _r Tb _a L _b M _c (I),

Wherein T is Mg, Ca, Sr or Ba; E is Mg, Ca, Ba, Ti, Cu, Zn, B, Al, In, Sn, Sb, Bi, Ga, Y, La or Lu; L is Li, Na or K; M is Ce, Pr, Nd, Pm, Sm, Eu, Gd, Dy, Ho, Er, Tm, Yb or Mn; and 1.4≦x≦2.6,0≦y≦0.5, 4.3≦z≦5.6 , 7.4≦r≦9, 0.01≦a≦0.5, 0≦b≦0.5,0≦c≦0.5.

In the phosphor powder represented by the formula (I), the Tb ion is a luminescent center. The phosphor powder is excited by excitation light absorbable by Tb ions, and has a radiation peak having a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably more than 50 nm.

The phosphor powder of the present invention may be excited by excitation light having a wavelength of from 120 to 700 nm, preferably from 200 to 700 nm, more preferably from 250 to 650 nm, still more preferably from 350 to 600 nm.

The phosphor powder of the present invention is excited by excitation light absorbable by Tb ions, and has an emission peak with a full width at half maximum of more than 20 nm, preferably an emission peak having a full width at half maximum of more than 25 nm; more preferably having a full width at half maximum Radiation peaks greater than 50 nm.

According to a specific embodiment of the present invention, the phosphor powder of the present invention is excited by excitation light of 120 to 700 nm and has an emission peak having a full width at half maximum of 20 nm to 150 nm. According to a specific embodiment of the present invention, the phosphor powder of the present invention is excited by excitation light having a wavelength of 120 to 700 nm, and has a half-height width of more than 20 nm, preferably more than 25 nm, more preferably more than 50 nm. In some aspects of these embodiments, the phosphor powder of the present invention is excited by excitation light having a wavelength of from 250 to 650 nm and has an emission peak having a full width at half maximum of greater than 20 nm, preferably greater than 25 nm, more preferably greater than 50 nm. In some aspects of these embodiments, the phosphor powder of the present invention is excited by excitation light having a wavelength of from 350 to 600 nm, and has a radiation peak having a full width at half maximum of greater than 20 nm, preferably greater than 25 nm, more preferably greater than 50 nm.

In general fluorescent powders, if strontium (Tb) ions are used as an activator, problems such as poor radiation peaks, poor efficiency, and lack of adjustability of light color are often affected, which affects their application value.

The phosphor powder of the present invention is excited by excitation light absorbable by Tb ions and has a broad emission peak in the luminescence spectrum. Therefore, the phosphor powder of the present invention can improve the lack of conventional fluorescent powder efficiency and the lack of adjustability of light color. According to a specific embodiment of the present invention, the phosphor powder of the present invention is excited by excitation light absorbable by Tb ions, and the light emission spectrum has an emission peak with a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably more than 50 nm. . According to an embodiment of the present invention, the phosphor powder of the present invention is excited by excitation light absorbable by Tb ions, and has an emission peak with a full width at half maximum of more than 20 nm in the yellow to red region, preferably greater than 25 nm. More preferably, it is greater than 50 nm.

The phosphor powder of the present invention is excited by excitation light absorbable by Tb ions and has a broad excitation peak. According to a specific embodiment of the invention, the phosphor powder is excited by excitation light absorbable by Tb ions, and has an excitation peak having a full width at half maximum of more than 50 nm, preferably more than 70 nm, more preferably more than 90 nm. According to a specific embodiment of the present invention, the phosphor powder of the present invention is excited by excitation light of 120 to 700 nm, and has an excitation peak having a full width at half maximum of more than 50 nm, preferably more than 70 nm, more preferably more than 90 nm. According to a specific embodiment of the invention, the phosphor powder has a broad excitation peak in the wavelength range of 350 to 600 nm, and the broad excitation peak has a wavelength greater than 50 nm, preferably greater than 70 nm, more preferably greater than 90 nm. height width.

According to an embodiment of the invention, the integral area of the excitation peak intensity of the phosphor powder having a wavelength of 350 to 600 nm is greater than the integral area of the excitation peak intensity of the wavelength of 200 to 350 nm. According to an embodiment of the invention, the integrated area of the excitation peak intensity of the phosphor powder having a wavelength of 350 to 600 nm is greater than 0.1 times the integral area of the excitation peak intensity of the wavelength of 200 to 350 nm. Preferably, the integrated area of the excitation peak intensity of the phosphor powder having a wavelength of 350 to 600 nm is greater than 0.2 times, more preferably more than 0.3 times, the integrated area of the excitation peak intensity of the wavelength of 200 to 350 nm.

The phosphor powder of the present invention has an average particle diameter of from 0.01 μm to 50 μm, preferably from 0.05 μm to 30 μm, more preferably from 0.1 μm to 10 μm.

According to an embodiment of the present invention, the phosphor powder represented by the formula (I) is represented by the following formula (I-1):

T _x Si _z N _r Tb _a (I-1),

Where T, x, z, r, a are as defined above.

In the phosphor powder represented by the formula (I-1), T is preferably Ca, Sr or Ba. The phosphor powder represented by the formula (I-1) is preferably composed of Sr, Si, N, and Tb. Examples of the phosphor powder represented by the formula (I-1) include, but are not limited to, Sr _1.4 Si _5.6 Tb _0.3 N _8.7 , Sr ₂ Si ₅ Tb _0.15 N _8.15 , Sr _2.6 Si _4.3 Tb _0.01 N _7.48 and Sr _1.88 Si ₅ Tb _0.08 N ₈ . According to a specific embodiment of the present invention, the phosphor powder represented by the formula (I-1) is excited by excitation light absorbable by Tb ions, and has a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably more than 50 nm. Radiation peak. In some aspects of the embodiments, the phosphor powder of the formula (I-1) is excited by excitation light having a wavelength of 250 to 600 nm, and has a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably It is a radiation peak greater than 50 nm. In some aspects of the embodiments, the phosphor powder of the formula (I-1) is excited by excitation light having a wavelength of 350 to 600 nm, and has a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably It is a radiation peak greater than 50 nm. According to an embodiment of the present invention, the phosphor powder of the formula (I-1) is excited by excitation light absorbable by Tb ions, and has an emission peak of a yellow to red region in the emission spectrum. According to an embodiment of the present invention, the phosphor powder represented by the formula (I-1) is excited by the excitation light absorbable by the Tb ion, and has an emission peak with a full width at half maximum of more than 20 nm in the yellow to red region. Preferably, it is greater than 25 nm, more preferably greater than 50 nm. According to an embodiment of the present invention, the phosphor powder of the formula (I-1) has a broad excitation peak in a wavelength range of 350 to 600 nm, and the broad excitation peak has a wavelength greater than 50 nm, preferably more than 70 nm. More preferably, it is half a height and width greater than 90 nm.

According to an embodiment of the present invention, the phosphor powder represented by the formula (I) is represented by the following formula (I-2):

T _x Si _z N _r Tb _a L _b (I-2),

Wherein T, L, x, z, r, a, b are as defined above.

In the phosphor powder represented by the formula (I-2), T is preferably Ca, Sr or Ba. The phosphor powder represented by the formula (I-2) is preferably composed of Ca, Sr or Ba, Si, N, Tb, and Li, Na or K. Examples of the phosphor powder represented by the formula (I-2) include, but are not limited to, Sr _1.94 Si ₅ Tb _0.03 Li _0.03 N ₈ , Sr _1.9 Si ₅ Tb _0.03 Li _0.03 N _7.97 , Ca _1.92 Si ₅ Tb _0.04 Li _0.04 N ₈ , Ba _1.92 Si ₅ Tb _0.04 Li _0.04 N ₈ , Sr _1.9 Si _5.1 Tb _0.1 K _0.15 N _8.22 and Sr ₂ Si _5.2 Tb _0.03 Na _0.3 N _8.4 . According to a specific embodiment of the present invention, the phosphor powder of the formula (I-2) is excited by excitation light absorbable by Tb ions, and has a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably more than 50 nm. Radiation peak. In some aspects of the embodiments, the phosphor powder of the formula (I-2) is excited by excitation light having a wavelength of 250 to 600 nm, and has a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably It is a radiation peak greater than 50 nm. In some aspects of the embodiments, the phosphor powder of the formula (I-2) is excited by excitation light having a wavelength of 350 to 600 nm, and has a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably It is a radiation peak greater than 50 nm. According to an embodiment of the present invention, the phosphor powder of the formula (I-2) is excited by excitation light absorbable by Tb ions, and has an emission peak of a yellow to red region in the emission spectrum. According to an embodiment of the present invention, the phosphor powder represented by the formula (I-2) is excited by the excitation light absorbable by the Tb ion, and has an emission peak with a full width at half maximum of more than 20 nm in the yellow to red region. Preferably, it is greater than 25 nm, more preferably greater than 50 nm. According to a specific embodiment of the present invention, the phosphor powder of the formula (I-2) has a broad excitation peak in a wavelength range of 350 to 600 nm, and the broad excitation peak has a wavelength greater than 50 nm, preferably more than 70 nm. More preferably, it is half a height and width greater than 90 nm.

According to an embodiment of the present invention, the phosphor powder represented by the formula (I) is a phosphor powder represented by the following formula (I-3):

T _x Si _z N _r Tb _a M _c (I-3),

Wherein T, M, x, z, r, a, c are as defined above.

In the phosphor powder represented by the formula (I-3), T is preferably Ca, Sr or Ba. In the phosphor powder represented by the formula (I-3), M is preferably Eu, Dy or Mn. The phosphor powder represented by the formula (I-3) is preferably composed of Sr, Si, N, Tb, and Eu, Dy or Mn. Examples of the phosphor powder represented by the formula (I-3) include, but are not limited to, Sr _2.5 Si _4.8 Tb _0.2 Mn _0.2 N _8.4 , Sr _2.4 Si _4.7 Tb _0.3 Dy _0.3 N _8.47 and Sr ₂ Si ₅ Tb _0.03 Eu _0.03 N _8.05 . According to a specific embodiment of the present invention, the phosphor powder represented by the formula (I-3) is excited by excitation light absorbable by Tb ions, and has a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably more than 50 nm. Radiation peak. In some aspects of the embodiments, the phosphor powder of the formula (I-3) is excited by excitation light having a wavelength of 250 to 600 nm, and has a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably It is a radiation peak greater than 50 nm. In some aspects of the embodiments, the phosphor powder of the formula (I-3) is excited by excitation light having a wavelength of 350 to 600 nm, and has a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably It is a radiation peak greater than 50 nm. According to an embodiment of the present invention, the phosphor powder of the formula (I-3) is excited by excitation light absorbable by Tb ions, and has an emission peak of a yellow to red region in the emission spectrum. According to an embodiment of the present invention, the phosphor powder represented by the formula (I-3) is excited by the excitation light absorbable by the Tb ion, and has an emission peak with a full width at half maximum of more than 20 nm in the yellow to red region. Preferably, it is greater than 25 nm, more preferably greater than 50 nm. According to an embodiment of the present invention, the phosphor powder of the formula (I-3) has a broad excitation peak in a wavelength range of 350 to 600 nm, and the broad excitation peak has a wavelength greater than 50 nm, preferably more than 70 nm. More preferably, it is half a height and width greater than 90 nm.

According to an embodiment of the present invention, the phosphor powder of the formula (I-4) shown in the formula (I) is as follows:

T _x E _y Si _z N _r Tb _a (I-4),

Wherein T, E, x, y, z, r, a are as defined above.

In the phosphor powder represented by the formula (I-4), T is preferably Ca, Sr or Ba. In the phosphor powder represented by the formula (I-4), E is preferably Ca, Ba or Bi. The phosphor powder represented by the formula (I-4) is preferably composed of Sr, Si, N, Tb, and Ca, Ba or Bi. Examples of the phosphor powder represented by the formula (I-4) include, but are not limited to, Sr _2.3 Si _4.9 Tb _0.08 Bi _0.02 N _8.17 , Sr _2.2 Ca _0.3 Si _5.2 Tb _0.1 N _8.7 , Sr _2.3 Ca _0.05 Si _4.8 Tb _0.25 N _8.22 , Sr _1.7 Ba _0.5 Si ₅ Tb _0.15 N _8.28 , Sr _1.9 Ba _0.1 Si _5.1 Tb _0.15 N _8.28 and Sr _1.5 Ba _0.05 Si _5.5 Tb _0.3 N _8.67 . According to a specific embodiment of the present invention, the phosphor powder represented by the formula (I-4) is excited by excitation light absorbable by Tb ions, and has a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably more than 50 nm. Radiation peak. In some aspects of the embodiments, the phosphor powder of the formula (I-4) is excited by excitation light having a wavelength of 250 to 600 nm, and has a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably It is a radiation peak greater than 50 nm. In some aspects of the embodiments, the phosphor powder of the formula (I-4) is excited by excitation light having a wavelength of 350 to 600 nm, and has a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably It is a radiation peak greater than 50 nm. According to an embodiment of the present invention, the phosphor powder of the formula (I-4) is excited by excitation light absorbable by Tb ions, and has an emission peak of a yellow to red region in the emission spectrum. According to an embodiment of the present invention, the phosphor powder represented by the formula (I-4) is excited by the excitation light absorbable by the Tb ion, and has an emission peak with a full width at half maximum of more than 20 nm in the yellow to red region. Preferably, it is greater than 25 nm, more preferably greater than 50 nm. According to a specific embodiment of the present invention, the phosphor powder of the formula (I-4) has a broad excitation peak in a wavelength range of 350 to 600 nm, and the broad excitation peak has a wavelength greater than 50 nm, preferably more than 70 nm. More preferably, it is half a height and width greater than 90 nm.

The phosphor powder of the present invention can be used as a red phosphor powder. The phosphor powder of the present invention is excited by excitation light absorbable by Tb ions, and has an emission peak of a yellow to red region in the emission spectrum. According to the invention, the luminescent color of the phosphor powder is red. According to an embodiment of the present invention, the phosphor powder of the formula (I) is excited by excitation light having a wavelength of 250 to 600 nm, and has an emission peak of a yellow to red region in the emission spectrum. According to an embodiment of the present invention, the phosphor powder of the formula (I) is excited by excitation light having a wavelength of 350 to 600 nm, and has an emission peak of a yellow to red region in the emission spectrum.

At present, many red fluorescent powders use Eu ³⁺ as an activator, and the radiation spectrum is sharp peak shape, the luminous efficiency is difficult to be improved, and the light color lacks adjustability.

The phosphor powder of the present invention is excited by excitation light absorbable by Tb ions, and has an emission peak having a full width at half maximum of more than 20 nm, preferably more than 25 nm, more preferably more than 50 nm. Therefore, the phosphor powder of the present invention can improve the lack of conventional fluorescent powder efficiency and the lack of adjustability of light color. According to the present invention, the phosphor powder is excited by excitation light having a wavelength of from 250 to 600 nm, and has an emission peak having a full width at half maximum of more than 20 nm in the luminescence spectrum, preferably more than 25 nm, more preferably more than 50 nm. According to the present invention, the phosphor powder is excited by excitation light having a wavelength of 350 to 600 nm, and has an emission peak having a full width at half maximum of more than 20 nm in the luminescence spectrum, preferably more than 25 nm, more preferably more than 50 nm.

According to an embodiment of the present invention, the phosphor powder represented by the formula (I-1) to the formula (I-4) is excited by excitation light having a wavelength of 250 to 600 nm, and has an emission peak having a full width at half maximum of more than 20 nm in the luminescence spectrum. Preferably, it is greater than 25 nm, more preferably greater than 50 nm. According to an embodiment of the present invention, the phosphor powder represented by the formula (I-1) to the formula (I-4) is excited by excitation light having a wavelength of 350 to 600 nm, and has an emission peak having a full width at half maximum of more than 20 nm in the luminescence spectrum. Preferably, it is greater than 25 nm, more preferably greater than 50 nm.

According to an embodiment of the invention, the formula Sr _1.4 Si _5.6 Tb _0.3 N _8.7 , Sr ₂ Si ₅ Tb _0.15 N _8.15 , Sr _2.6 Si _4.3 Tb _0.01 N _7.48 , Sr _1.88 Si ₅ Tb _0.08 N ₈ , Sr _1.94 Si ₅ Tb _0.03 Li _0.03 N ₈ , Sr _1.9 Si ₅ Tb _0.03 Li _0.03 N _7.97 , Ca _1.92 Si ₅ Tb _0.04 Li _0.04 N ₈ , Ba _1.92 Si ₅ Tb _0.04 Li _0.04 N ₈ , Sr _1.9 Si _5.1 Tb _0.1 K _0.15 N _8.22 , Sr ₂ Si _5.2 Tb _0.03 Na _0.3 N _8.4 , Sr _2.5 Si _4.8 Tb _0.2 Mn _0.2 N _8.4 , Sr _2.4 Si _4.7 Tb _0.3 Dy _0.3 N _8.47 , Sr ₂ Si ₅ Tb _0.03 Eu _0.03 N _8.05 , Sr _2.3 Si _4.9 Tb _0.08 Bi _0.02 N _8.17 , Sr _2.2 Ca _0.3 Si _5.2 Tb _0.1 N _8.7 , Sr _2.3 Ca _0.05 Si _4.8 Tb _0.25 N _8.22 , Sr _1.7 Ba _0.5 Si ₅ Tb _0.15 N _8.28 , Sr _1.9 Ba _0.1 Si _5.1 Tb _0.15 N _8.28 , Sr _1.5 Ba _0.05 Si _5.5 Tb _0.3 N _8.67 The phosphor powder is excited by excitation light having a wavelength of 250 to 600 nm, preferably excited by excitation light having a wavelength of 350 to 600 nm, and having a half-height width of more than 20 nm in the emission spectrum. The peak is preferably greater than 25 nm, more preferably greater than 50 nm.

The phosphor powder of the present invention may optionally contain additional co-activators and/or sensitizers. A co-activator, a sensitizer, which is well known in the art, may be used and will not be described again.

The fluorescent powder of the present invention can be produced by any conventional phosphor powder preparation technique, such as, but not limited to, solid state method, sol-gel method, and coprecipitation method. (co-precipitation method), combustion synthesis method, hydrothermal method, chemical vapor method, physical vapor deposition method, and the like. Among them, the solid phase method uses a dry mixing or a wet mixing method to mix raw materials, and then calcination/sintering at a high temperature to obtain a fluorescent powder. When the phosphor powder is prepared by the solid phase method, a fluxing agent may be added as needed.

The elemental raw material used for preparing the phosphor powder of the present invention includes a metal or a compound containing the element. Examples of the compound include, but are not limited to, oxides, nitrides, sulfides, carbides, halogen compounds, carbonates, nitrates, oxalates, sulfates, organic salts, and the like. The elemental material used can be used as an activator, sensitizer and/or charge compensator for the phosphor powder. According to an embodiment of the present invention, when the phosphor powder is synthesized by using Sr ions and Tb ions, since the valence of the Sr ion is divalent, and the valence of the Tb ion is trivalent or tetravalent, the non-divalent ion can be added by adding For example, alkali metal group ions (Li, Na, K, Rb, Cs) are subjected to valence charge compensation to improve the luminous efficiency of the powder.

According to an embodiment of the present invention, the phosphor powder of the present invention can be prepared using a solid phase method. In a partial aspect, the raw materials required for preparing the phosphor powder of the present invention are uniformly mixed, and then subjected to a heating reaction. The heating temperature is from 1000 ° C to 1800 ° C, preferably from 1100 ° C to 1700 ° C, more preferably from 1200 ° C to 1600 ° C. The heating time is from 0.5 hours to 72 hours, preferably from 1 hour to 60 hours, more preferably from 1.5 hours to 48 hours. The heating pressure is from 0.3 atm to 15 atm, preferably from 0.5 atm to 10 atm, more preferably from 0.7 atm to 5 atm. The heating reaction is carried out in an atmosphere capable of reducing the ability to change the bonding environment around the Tb ions, thereby changing the light-emitting properties. The atmosphere contains hydrogen, ammonia, methane, carbon monoxide and/or other carbonaceous elements, and the atmosphere may contain other gases such as nitrogen, argon, and the like.

A fluxing aid may be used as needed to prepare the phosphor powder. By adding a fluxing agent, the sintering reaction of the powder can be promoted and the desired reaction temperature can be lowered. Examples of the fluxing agent include, but are not limited to, AlF ₃ , B ₂ O ₃ , H ₃ BO ₃ , BaO, BaCl ₂ , BaF ₂ , Bi ₂ O ₃ , CaHPO ₄ , CaF ₂ , CaSO ₄ , LiF, Li ₂ O, Li ₂ CO ₃ , LiNO ₃ , K ₂ O, KF, KCl, MgF ₂ , MoO ₃ , NaCl, Na ₂ O, NaF, Na ₃ AlF ₆ , NH ₄ F, NH ₄ Cl, (NH ₄ ) ₂ HPO ₄ , SrF ₂ , SrS, CaS, SrSO ₄ , SrHPO ₄ , PbO, PbF ₂ , WO ₃ , urea, glucose, other low melting point materials, and combinations thereof.

The phosphor powder prepared by the solid phase method may be further ground as needed. Examples of the preparation of the phosphor powder of the present invention by the solid phase method are as described in the following examples, but are not limited thereto.

The phosphor powder of the present invention can be used for a light-emitting device such as, but not limited to, a photoluminescence device, an electroluminescence device, a cathode ray illuminating device, and the like. The phosphor powder of the present invention is excited by excitation light and has a broad radiation peak. Therefore, the lack of efficiency of the conventional phosphor powder and the lack of adjustability of the light color can be improved, which is in line with the needs of the industry. According to a specific embodiment of the present invention, the phosphor powder of the present invention can be used in a photoluminescence device. In accordance with an embodiment of the present invention, the phosphor powder of the present invention can be used in a light emitting diode such as, but not limited to, a blue light excitation or a UV light excitation light emitting diode. According to a specific embodiment of the present invention, the phosphor powder of the present invention can be used for a white light emitting diode. In addition, the phosphor powder of the present invention may be used alone or in combination with other phosphor powders such as, but not limited to, yellow phosphor powder, blue phosphor powder, green phosphor powder, and/or Other red fluorescent powders are used in combination.

The present invention provides a light-emitting device having a phosphor powder as shown in the above formula (I). The light emitting device can be, for example, but not limited to, a photoluminescent device, an electroluminescent device, a cathode ray emitting device, and the like. According to a specific embodiment of the invention, the illumination device of the invention is a photoluminescence device. According to the present invention, the phosphor powder in the light-emitting device is excited by excitation light and has a broad radiation peak, thereby improving the efficiency of the conventional phosphor powder and the lack of adjustability of the light color, which is in line with the industry. demand. In general, a light emitting device can include, for example, a light source (eg, an LED wafer (eg, a blue LED wafer)) and a phosphor powder, wherein the phosphor system is excited by excitation light from a light source. According to a specific embodiment of the present invention, the light-emitting device of the present invention is a light-emitting diode, such as, but not limited to, a blue light-excited or UV-light-excited light-emitting diode. In some aspects of these embodiments, the illumination device comprises a blue light source and a phosphor powder. According to an embodiment of the invention, the illumination device of the invention is a white light emitting diode. In addition, in the light-emitting device, the phosphor powder of the present invention may be used alone or in combination with other phosphor powders such as, but not limited to, yellow phosphor powder, blue phosphor powder, and green phosphor. Powder and/or other red fluorescent powders are used in combination.

The light-emitting device of the present invention can be applied to general illumination, display illumination (such as traffic signs), medical device illumination, automotive electronic equipment, and the like. The illuminating device of the present invention is also applicable to an LCD (Liquid Crystal Display) backlight, and can be applied to a display (such as a mobile phone, a digital camera, a television, a computer screen, etc.).

The invention will be more specifically described by the examples, but these examples are not intended to limit the scope of the invention. Unless otherwise specified, the "%" and "parts by weight" used in the following examples and comparative examples to indicate the content of any component and the amount of any substance are based on the weight.

Example Example 1: Preparation and Analysis of Sr _1.94 Si ₅ Tb _0.03 Li _0.03 N ₈ Fluorescent Powder

Sr _1.94 Si ₅ Tb _0.03 Li _0.03 N ₈ phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , Si ₃ N ₄ , Tb ₄ O ₇ and Li ₃ N powders were weighed according to the cation ratio of the chemical formula. The glove box was uniformly mixed; then, calcination was carried out under a reducing atmosphere in which nitrogen and hydrogen were mixed, and the calcination temperature was 1400 ° C for 6 hours to obtain a phosphor powder of Sr _1.94 Si ₅ Tb _0.03 Li _0.03 N ₈ . The phosphor powder was analyzed by X-ray diffraction (XRD) to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 270 nm absorbable by Tb ions to produce a broad emission peak with a peak at 620 nm, and the half-height width of the emission peak was 96 nm, and the emission spectrum was as shown in Fig. 1. The integrated region of the excitation spectrum in the range of 350-600 nm is 1.06 times the integrated area in the range of 200-350 nm, and the excitation spectrum is as shown in FIG. 2, and has a broad excitation peak with a full width at half maximum of more than 120 nm between 350 and 600 nm. .

Example 2: Preparation and Analysis of Sr _1.4 Si _5.6 Tb _0.3 N _8.7 Fluorescent Powder

Sr _1.4 Si _5.6 Tb _0.3 N _8.7 phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , Si ₃ N ₄ and Tb ₄ O ₇ powders were weighed according to the cation ratio of the chemical formula, and uniformly mixed in a glove box; Subsequently, calcination was carried out under a reducing atmosphere in which nitrogen and hydrogen were mixed, and the calcination temperature was 1500 ° C for 6 hours to obtain a phosphor powder of Sr _1.4 Si _5.6 Tb _0.3 N _8.7 . The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions to produce a broad emission peak with a peak at 607 nm, and the half-height width of the emission peak was 86 nm, and the emission spectrum was as shown in Fig. 3.

Example 3: Preparation and Analysis of Sr ₂ Si ₅ Tb _0.15 N _8.15 Fluorescent Powder

Sr ₂ Si ₅ Tb _0.15 N _8.15 phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , Si ₃ N ₄ and Tb ₄ O ₇ powders were weighed according to the cation ratio of the chemical formula, and uniformly mixed in a glove box; Subsequently, calcination was carried out under a reducing atmosphere in which nitrogen and hydrogen were mixed, and the calcination temperature was 1500 ° C for 6 hours to obtain a phosphor powder of Sr ₂ Si ₅ Tb _0.15 N _8.15 . The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions, and a broad emission peak with a peak at 608 nm was generated, and the half width of the radiation peak was 86 nm, and the luminescence spectrum thereof was as shown in Fig. 4.

Example 4: Preparation and Analysis of Sr _2.6 Si _4.3 Tb _0.01 N _7.48 Fluorescent Powder

Sr _2.6 Si _4.3 Tb _0.01 N _7.48 phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , Si ₃ N ₄ and Tb ₄ O ₇ powders were weighed according to the cation ratio of the chemical formula, and uniformly mixed in a glove box; Subsequently, calcination was carried out under a reducing atmosphere in which nitrogen and hydrogen were mixed, and the calcination temperature was 1500 ° C for 6 hours to obtain a phosphor powder of Sr _2.6 Si _4.3 Tb _0.01 N _7.48 . The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions, resulting in a broad emission peak with a peak at 609 nm, and a half-height width of the emission peak of 87 nm.

Example 5: Preparation and Analysis of Sr _1.9 Si ₅ Tb _0.03 Li _0.03 N _7.97 Fluorescent Powder

Sr _1.9 Si ₅ Tb _0.03 Li _0.03 N _7.97 phosphor was prepared by solid phase method, and Sr ₃ N ₂ , Si ₃ N ₄ , Tb ₄ O ₇ and LiF powders were weighed in the glove box according to the cation ratio of the chemical formula. The mixture was uniformly mixed; then, calcination was carried out under a reducing atmosphere in which nitrogen and hydrogen were mixed, and the calcination temperature was 1,450 ° C for 6 hours to obtain a phosphor powder of Sr _1.9 Si ₅ Tb _0.03 Li _0.03 N _7.97 . The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions, and a broad emission peak with a peak at 613 nm was generated, and the half width of the radiation peak was 88 nm.

Example 6: Preparation and Analysis of Sr _1.9 Si _5.1 Tb _0.1 K _0.15 N _8.22 Fluorescent Powder

Sr _1.9 Si _5.1 Tb _0.1 K _0.15 N _8.22 phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , Si ₃ N ₄ , Tb ₄ O ₇ and KCl powders were weighed according to the cation ratio of the chemical formula. The mixture was uniformly mixed; then, calcination was carried out under a reducing atmosphere in which nitrogen and hydrogen were mixed, and the calcination temperature was 1600 ° C for 4 hours to obtain a phosphor powder of Sr _1.9 Si _5.1 Tb _0.1 K _0.15 N _8.22 . The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions to produce a broad emission peak with a peak at 610 nm, and a half-height width of the emission peak of 86 nm.

Example 7: Preparation and Analysis of Sr ₂ Si _5.2 Tb _0.03 Na _0.3 N _8.4 Fluorescent Powder

Sr ₂ Si _5.2 Tb _0.03 Na _0.3 N _8.4 fluorescein powder was prepared by solid phase method, and Sr ₃ N ₂ , Si ₃ N ₄ , Tb ₄ O ₇ and NaCl powders were weighed according to the cation ratio of the chemical formula. The mixture was uniformly mixed; then, calcination was carried out under a reducing atmosphere in which nitrogen and hydrogen were mixed, and the calcination temperature was 1600 ° C for 4 hours to obtain a phosphor powder of Sr ₂ Si _5.2 Tb _0.03 Na _0.3 N _8.4 . The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions, and a broad emission peak with a peak at 610 nm was generated, and the half-height width of the emission peak was 87 nm.

Example 8: Preparation and Analysis of Sr _2.3 Si _4.9 Tb _0.08 Bi _0.02 N _8.17 Fluorescent Powder

Sr _2.3 Si _4.9 Tb _0.08 Bi _0.02 N _8.17 phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , Si ₃ N ₄ , Tb ₄ O ₇ and Bi ₂ O ₃ powders were _weighed according to the cation ratio of the chemical formula. The mixture was uniformly mixed in a glove box; then, calcination was carried out under a reducing atmosphere in which nitrogen and hydrogen were mixed, and the calcination temperature was 1600 ° C for 4 hours to obtain a phosphor powder of Sr _2.3 Si _4.9 Tb _0.08 Bi _0.02 N _8.17 . The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions, resulting in a broad emission peak with a peak at 607 nm, and a half-height width of the emission peak of 84 nm.

Example 9: Preparation and Analysis of Sr _2.5 Si _4.8 Tb _0.2 Mn _0.2 N _8.4 Fluorescent Powder

Sr _2.5 Si _4.8 Tb _0.2 Mn _0.2 N _8.4 phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , Si ₃ N ₄ , Tb ₄ O ₇ and Mn ₂ O ₃ powders were weighed according to the cation ratio of the chemical formula. Uniformly mixed in a glove box; then, calcined under a reducing atmosphere of 95% nitrogen and 5% hydrogen, and calcined at 1600 ° C for 4 hours to obtain Sr _2.5 Si _4.8 Tb _0.2 Mn _0.2 N _8.4 Light powder. The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions, resulting in a broad emission peak with a peak at 612 nm, and a half-height width of the emission peak of 85 nm.

Example 10: Preparation and Analysis of Sr _2.4 Si _4.7 Tb _0.3 Dy _0.3 N _8.47 Fluorescent Powder

Sr _2.4 Si _4.7 Tb _0.3 Dy _0.3 N _8.47 phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , Si ₃ N ₄ , Tb ₄ O ₇ and Dy ₂ O ₃ powders were _weighed according to the cation ratio of the chemical formula. The mixture was uniformly mixed in a glove box; then, calcination was carried out under a reducing atmosphere in which nitrogen and hydrogen were mixed, and the calcination temperature was 1600 ° C for 4 hours to obtain a phosphor powder of Sr _2.4 Si _4.7 Tb _0.3 Dy _0.3 N _8.47 . The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions to produce a broad emission peak with a peak at 620 nm, and a half-height width of the emission peak of 93 nm.

Example 11: Preparation and Analysis of Sr ₂ Si ₅ Tb _0.03 Eu _0.03 N _8.05 Fluorescent Powder

Sr ₂ Si ₅ Tb _0.03 Eu _0.03 N _8.05 phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , Si ₃ N ₄ , Tb ₄ O ₇ and Eu ₂ O ₃ powders were _weighed according to the cation ratio of the chemical formula. The mixture was uniformly mixed in a glove box; then, calcination was carried out under a reducing atmosphere in which nitrogen and hydrogen were mixed, and the calcination temperature was 1,450 ° C for 6 hours to obtain a phosphor powder of Sr ₂ Si ₅ Tb _0.03 Eu _0.03 N _8.05 . The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions, resulting in a broad emission peak with a peak at 620 nm, and a half-height width of the emission peak of 90 nm.

Example 12: Preparation and Analysis of Sr _2.2 Ca _0.3 Si _5.2 Tb _0.1 N _8.7 Fluorescent Powder

Sr _2.2 Ca _0.3 Si _5.2 Tb _0.1 N _8.7 (6 wt% (wt%) H ₃ BO ₃ ) phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , CaO, Si _{3 were} weighed according to the cation ratio of the chemical formula. N ₄ , Tb ₄ O ₇ powder, adding 6 wt% of the fluxing agent H ₃ BO ₃ , uniformly mixed in a glove box according to the total weight of the reactants; then, calcining under a reducing atmosphere of mixing nitrogen and hydrogen The calcination temperature was 1400 ° C for 8 hours, and a phosphor powder of Sr _2.2 Ca _0.3 Si _5.2 Tb _0.1 N _8.7 (6 wt% H ₃ BO ₃ ) was obtained. The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions to produce a broad emission peak with a peak at 608 nm, and a half-height width of the emission peak of 73 nm.

Example 13: Preparation and Analysis of Sr _1.7 Ba _0.5 Si ₅ Tb _0.15 N _8.28 Fluorescent Powder

Sr _1.7 Ba _0.5 Si ₅ Tb _0.15 N _8.28 (10 wt% NH ₄ Cl) phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , Ba ₃ N ₂ and Si ₃ N _{4 were} weighed according to the cation ratio of the chemical formula. , Tb ₄ O ₇ powder, based on the total weight of the reactants, adding 10% by weight of the fluxing agent NH ₄ Cl, uniformly mixed in the glove box; then, under the reducing atmosphere of nitrogen and hydrogen mixed, simmering, simmering The temperature was 1400 ° C for 8 hours, and a phosphor powder of Sr _1.7 Ba _0.5 Si ₅ Tb _0.15 N _8.28 (10 wt% NH ₄ Cl) was obtained. The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions, resulting in a broad emission peak with a peak at 607 nm, and a half-height width of the emission peak of 78 nm.

Example 14: Preparation and Analysis of Sr _2.3 Ca _0.05 Si _4.8 Tb _0.25 N _8.22 Fluorescent Powder

Sr _2.3 Ca _0.05 Si _4.8 Tb _0.25 N _8.22 (2 wt% NH ₄ F) phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , CaO, Si ₃ N ₄ and Tb _{4 were} weighed according to the cationic ratio of the chemical formula. O ₇ powder, adding 2 wt% of the fluxing agent NH ₄ F, uniformly mixed in a glove box according to the total weight of the reactants; then, calcining under a reducing atmosphere of mixing nitrogen and hydrogen, the calcination temperature is 1400 At 90 °, a fluorescent powder of Sr _2.3 Ca _0.05 Si _4.8 Tb _0.25 N _8.22 (2 wt% NH ₄ F) was obtained over 8 hours. The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor at 420 nm absorbable by Tb ions, resulting in a broad emission peak with a peak at 608 nm and a half-height width of the emission peak of 84 nm.

Example 15: Preparation and Analysis of Sr _1.9 Ba _0.1 Si _5.1 Tb _0.15 N _8.28 Fluorescent Powder

Sr _1.9 Ba _0.1 Si _5.1 Tb _0.15 N _8.28 (3 wt% H ₃ BO ₃ ) phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , Ba ₃ N ₂ , Si ₃ N were weighed according to the cation ratio of the chemical formula. ₄ , Tb ₄ O ₇ powder, based on the total weight of the reactants, adding 3 wt% of the fluxing agent H ₃ BO ₃ , uniformly mixed in the glove box; then, under the reducing atmosphere of nitrogen and hydrogen mixed, simmering, The calcination temperature was 1400 ° C for 8 hours, and a phosphor powder of Sr _1.9 Ba _0.1 Si _5.1 Tb _0.15 N _8.28 (3 wt% H ₃ BO ₃ ) was obtained. The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor at 420 nm at which Tb ions can be absorbed, resulting in a broad emission peak with a peak at 611 nm, and a half-height width of the emission peak of 87 nm.

Example 16: Preparation and Analysis of Sr _1.5 Ba _0.05 Si _5.5 Tb _0.3 N _8.67 Fluorescent Powder

Sr _1.5 Ba _0.05 Si _5.5 Tb _0.3 N _8.67 (4 wt% NH ₄ Cl) phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , Ba ₃ N ₂ and Si ₃ N _{4 were} weighed according to the cation ratio of the chemical formula. , Tb ₄ O ₇ powder, based on the total weight of the reactants, adding 4 wt% of the fluxing agent NH ₄ Cl, uniformly mixed in the glove box; then, under the reducing atmosphere of nitrogen and hydrogen mixed, simmering, simmering The temperature was 1400 ° C for 8 hours, and a phosphor powder of Sr _1.5 Ba _0.05 Si _5.5 Tb _0.3 N _8.67 (4 wt% NH ₄ Cl) was obtained. The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor at 420 nm at which Tb ions can be absorbed, resulting in a broad emission peak with a peak at 608 nm, and a half-height width of the emission peak of 85 nm.

Example 17: Preparation and Analysis of Sr _1.88 Si ₅ Tb _0.08 N ₈ Fluorescent Powder

Sr _1.88 Si ₅ Tb _0.08 N ₈ phosphor powder was prepared by solid phase method, and Sr ₃ N ₂ , Si ₃ N ₄ and TbCl ₃ powders were weighed according to the cation ratio of the chemical formula, and uniformly mixed in a glove box; The calcination was carried out under a reducing atmosphere in which nitrogen and hydrogen were mixed, and the calcination temperature was 1200 ° C for 2 hours to obtain a phosphor powder of Sr _1.88 Si ₅ Tb _0.08 N ₈ . The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions, resulting in a broad emission peak with a peak at 606 nm, and a half-height width of the emission peak of 84 nm.

Example 18: Preparation and Analysis of Ca _1.92 Si ₅ Tb _0.04 Li _0.04 N ₈ Fluorescent Powder

Ca _1.92 Si ₅ Tb _0.04 Li _0.04 N ₈ phosphor powder was prepared by solid phase method, and CaH ₂ , Si ₃ N ₄ , Tb ₂ O ₃ and Li ₃ N powders were weighed according to the cation ratio of the chemical formula. The mixture was uniformly mixed; then, calcination was carried out under a reducing atmosphere in which nitrogen and hydrogen were mixed, and the calcination temperature was 1500 ° C for 4 hours to obtain a phosphor powder of Ca _1.92 Si ₅ Tb _0.04 Li _0.04 N ₈ . The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Ca ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions to produce a broad emission peak with a peak at 603 nm, and a half-height width of the emission peak of 99 nm.

Example 19: Preparation and Analysis of Ba _1.92 Si ₅ Tb _0.04 Li _0.04 N ₈ Fluorescent Powder

Ba _1.92 Si ₅ Tb _0.04 Li _0.04 N ₈ phosphor powder was prepared by solid phase method, and Ba ₃ N ₂ , Si ₃ N ₄ , TbCl ₃ and Li ₃ N powders were weighed according to the cation ratio of the chemical formula. The mixture was uniformly mixed; then, calcination was carried out under a reducing atmosphere in which nitrogen and hydrogen were mixed, and the calcination temperature was 1,250 ° C for 4 hours to obtain a phosphor powder of Ba _1.92 Si ₅ Tb _0.04 Li _0.04 N ₈ . The phosphor powder was confirmed by XRD analysis to confirm that the crystal bulk structure was Sr ₂ Si ₅ N ₈ . Fluorescence spectrometer analysis was carried out to excite the phosphor powder at 420 nm absorbable by Tb ions to produce a broad emission peak with a peak at 580 nm, and a half-height width of the emission peak of 85 nm.

Example 20

The phosphor powders Sr _1.94 Si ₅ Tb _0.03 Li _0.03 N ₈ , Sr ₂ Si ₅ Tb _0.03 Eu _0.03 N _8.05 , Sr _1.7 Ba _0.5 Si ₅ Tb _0.15 N _8.28 synthesized by the examples 1, ₁₁ , ₁₃ , and ₁₈ , respectively. Ca _1.92 Si ₅ Tb _0.04 Li _0.04 N ₈ is mixed with an oxy-resin and packaged on a blue LED having a blue light wavelength of 460 nm. After the packaged LED test, the blue light wafer can excite the encapsulated phosphor powder to generate red light, and the blue light of the wafer is mixed with the red light of the fluorescent material to display a purple-red light, which proves the compatibility of the fluorescent material of the invention with the blue LED. .

The phosphor powder of the invention is excited by excitation light, has a broad radiation peak, can improve the lack of efficiency of the conventional phosphor powder and the lack of adjustability of the light color, and has good thermal stability and good chemical stability. Excellent performance such as non-toxicity and high strength, which is in line with the needs of the industry.

The above examples are merely illustrative of the compositions and preparation methods of the present invention and are not intended to limit the invention. Modifications and variations of the above-described embodiments can be made by those skilled in the art without departing from the spirit and scope of the invention. Therefore, the scope of the claims of the present invention should be as set forth in the appended claims.

1 is an emission spectrum of a Sr _1.94 Si ₅ Tb _0.03 Li _0.03 N ₈ phosphor powder according to an embodiment of the present invention;

2 is an excitation spectrum of a Sr _1.94 Si ₅ Tb _0.03 Li _0.03 N ₈ phosphor powder according to an embodiment of the present invention;

Figure 3 is a graph showing the luminescence spectrum of a Sr _1.4 Si _5.6 Tb _0.3 N _8.7 phosphor powder according to an embodiment of the present invention;

Figure 4 is a graph showing the luminescence spectrum of Sr ₂ Si ₅ Tb _0.15 N _8.15 phosphor powder according to an embodiment of the present invention.

Claims (16)

A phosphor powder comprising an alkaline earth ion, a Si ion, an N ion and a Tb ion, wherein the Tb ion is an illuminating center, and the phosphor powder is excited by an excitation light absorbable by Tb ions, and has a full width at half maximum of more than 20 nm. Radiation peak. The phosphor powder according to claim 1, wherein the alkaline earth ion is Mg ion, Ca ion, Sr ion, Ba ion or a combination thereof. The phosphor powder according to the first aspect of the patent application includes Mg ions, Ca ions, Sr ions, Ba ions, Ti ions, Cu ions, Zn ions, B ions, Al ions, In ions, Sn ions, Sb, Bi, Ga, Y, La, Lu, Li, Na, K, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Dy Ho ion, Er ion, Tm ion, Yb ion, Mn ion or a combination thereof. The fluorescent powder according to claim 1, wherein the fluorescent powder is represented by the formula (I): T _x E _y Si _z N _r Tb _a L _b M _c (I), wherein T is Mg, Ca , Sr or Ba; E is Mg, Ca, Ba, Ti, Cu, Zn, B, Al, In, Sn, Sb, Bi, Ga, Y, La or Lu; L is Li, Na or K; M is Ce , Pr, Nd, Pm, Sm, Eu, Gd, Dy, Ho, Er, Tm, Yb or Mn; 1.4≦x≦2.6,0≦y≦0.5, 4.3≦z≦5.6,7.4≦r≦9,0.01 ≦a≦0.5,0≦b≦0.5,0≦c≦0.5; and wherein, the Tb ion is an illuminating center, and the phosphor powder is excited by excitation light absorbable by Tb ions, and has a full width at half maximum of more than 20 nm. Radiation peak. The phosphor powder according to claim 4, wherein the phosphor powder is excited by excitation light absorbable by Tb ions, and has a radiation peak having a full width at half maximum of more than 25 nm. The phosphor powder according to claim 4, wherein the phosphor powder is excited by excitation light having a wavelength of 350 to 600 nm and has an emission peak having a full width at half maximum of more than 20 nm. The phosphor powder according to claim 4, wherein the phosphor powder has an excitation peak having a full width at half maximum of more than 50 nm in a wavelength range of 350 to 600 nm. The phosphor powder according to claim 4, wherein the integral area of the excitation peak intensity of the phosphor powder having a wavelength of 350 to 600 nm is greater than 0.1 times the integral area of the excitation peak intensity of the wavelength of 200 to 350 nm. The phosphor powder according to claim 4, wherein the preparation of the phosphor powder comprises a synthesis reaction carried out in a reducing atmosphere at a temperature greater than 1100 °C. The phosphor powder according to claim 4, wherein the phosphor powder has an average particle diameter of from 0.01 μm to 50 μm. The phosphor powder according to claim 4, which has the formula T _x Si _z N _r Tb _a . The phosphor powder according to claim 4, which has the formula T _x Si _z N _r Tb _a L _b . The phosphor powder according to claim 4, which has the formula T _x Si _z N _r Tb _a M _c . The phosphor powder according to claim 4, which has the formula T _x E _y Si _z N _r Tb _a . A light-emitting device having the phosphor powder according to any one of claims 1 to 14. The light-emitting device of claim 15, which is a light-emitting diode.